反应详情

Combine 5-nitro-2-pyrrolidin-1-yl-pyridine (5.6 g, 29 mmol), palladium hydroxide (1.96 g, 35 wt. %), ammonium formate (9.1 g, 145 mmol), 1N HCl/Et2O (41 ml), in methanol (289 ml) and stir. Heat reaction mixture to reflux for 1 hour. Cool reaction mixture and add carbon to decolorize. Filter the solution through celite, add 50 ml of saturated NaHCO3, and evaporate in vacuo to remove the methanol and ether. Extract the residue 3 times into CH2Cl2 from saturated NaHCO3, dry over Na2SO4, and evaporate in vacuo to obtain 6-pyrrolidin-1-yl-pyridin-3-ylamine. Mass spec.: M+1=164 (AP+). C. 1′-(6-pyrrolidin-pyridin-3-yl-carbamoyl)-spiroisobenzofuran-1,4′4′-piperidine

1. temperatureHeat
2. customreaction mixture
3. temperatureto reflux for 1 hour
4. temperatureCool
5. customreaction mixture
6. additionadd carbon
7. filtrationFilter the solution through celite
8. additionadd 50 ml of saturated NaHCO3
9. customevaporate in vacuo
10. customto remove the methanol and ether
11. extractionExtract the residue 3 times into CH2Cl2 from saturated NaHCO3
12. dry with materialdry over Na2SO4
13. customevaporate in vacuo